CN105131881A - Conductive silver adhesive with low solid content and capable of being rapidly cured at medium and normal temperature - Google Patents

Conductive silver adhesive with low solid content and capable of being rapidly cured at medium and normal temperature Download PDF

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Publication number
CN105131881A
CN105131881A CN201510646972.2A CN201510646972A CN105131881A CN 105131881 A CN105131881 A CN 105131881A CN 201510646972 A CN201510646972 A CN 201510646972A CN 105131881 A CN105131881 A CN 105131881A
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conductive silver
present
silver glue
glue according
conductive
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CN105131881B (en
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阮海波
王然龙
李璐
刘碧桃
关有为
黎军军
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Shanghai Juerxi Electronic Technology Co ltd
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Chongqing University of Arts and Sciences
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Abstract

The invention discloses a conductive silver adhesive with low solid content and capable of being rapidly cured at medium and normal temperature. The conductive silver adhesive is prepared from 1%-2% of silver nanowires, 13%-29% of flake silver powder, 20%-30% of bisphenol A epoxy resin, 5%-10% of rapid medium and normal temperature curing agents, 0.5%-1% of rapid medium and normal temperature curing accelerant, 1%-3% of thinning agents, 1%-3% of K-570 or K-550, 0.5%-1% of terephthalic acid, 20%-56.3% of cellulose, 0.5%-1% of nano-silicon dioxide, 0.1%-0.5% of antifoaming agents and 0.1%-0.5% of ICAM8401 or ICAM8402. The conductive silver adhesive can be rapidly cured at medium and normal temperature and is low in silver content and low in cost, and therefore the application range of the conductive silver adhesive is greatly extended.

Description

A kind of quick-setting conductive silver glue of middle normal temperature of low-solid content
Technical field
The invention belongs to conductive resin field, be specifically related to a kind of quick-setting conductive silver glue of middle normal temperature of low-solid content.
Background technology
In the past, between two kinds of objects, build conductive path to realize mainly through tin lead welding.But the heavy metal contamination that tin lead welding produces and its higher welding temperature cause being restricted in the application of electronic information field.For addressing this problem, be developed conductive silver glue.Conductive silver glue is easy to use, excellent performance, contaminative are little, thus replaces the partial function of tin lead welding gradually at electronic information field and becomes a kind of important circuits built material, is widely used in microelectronics assembling, printed electronic circuit, bonding etc.The increase of demand have stimulated the research of conductive silver glue.
Patent CN104017529A uses the conductive silver glue of ten kinds of material allotments such as epoxy resin, silver powder, solidifying agent to have good cohesiveness, electrical and thermal conductivity and stability.But the same with most of conductive silver glue, the solidification value that this conductive silver glue is higher is unfavorable for that it is in market application such as flexibility wearings.For addressing this problem, patent CN104449455A develops the conductive silver glue of intermediate temperature setting, and its solidification value, lower than 100 DEG C, extends elargol range of application.But the elargol of these two Patent exploitations needs longer set time, can not meet the quick-setting requirement of the occasions such as streamline.Patent CN103642420A has prepared a kind of quick-setting thermoset conductive silver glue, solves this problem.But the conductive silver glue of excellent performance should have good cohesiveness and electroconductibility, not too high solidification value, shorter set time etc., should reduce the content (silver content of substantially all conductive silver glues is all at about 60-70%) of the higher silver of cost simultaneously simultaneously as far as possible.It's a pity, can meet these four conductive silver glues required also does not have simultaneously substantially.
For this reason, select suitable auxiliary agent to realize good elargol function and lower silver content is the problem that solution is needed in conductive silver glue field badly as far as possible.
Summary of the invention
The invention reside in the quick-setting conductive silver glue of middle normal temperature that a kind of low-solid content is provided, to solve the problem that current conductive silver glue fails to realize good electroconductibility, not too high solidification value, shorter set time and lower silver content simultaneously.Conductive silver glue prepared by the present invention and substrate have that good bonding force, conductivity are excellent, solidification value lower than 100 DEG C, that set time is less than half an hour, silver content lower (15-30%), stably stored time is long, can be widely used in numerous areas.The formula of this conductive silver glue is:
Nano silver wire, 1-2%;
Flake silver powder, 13-29%;
Bisphenol A epoxide resin, 20-30%;
Ambient cure agent fast, 5-10%;
Ambient cure promotor fast, 0.5-1%;
Thinner, 1-3%;
K-570 or K-550,1-3%;
Terephthalic acid, 0.5-1%;
Mierocrystalline cellulose, 20-56.3%;
Nano silicon, 0.5-1%;
Defoamer, 0.1-0.5%;
ICAM8401 or 8402,0.1-0.5%;
The length of the present invention's nano silver wire used is 30-50 μm, and diameter is 30-50nm.Flake silver powder used is 10 μm of silver powder;
The present invention's bisphenol A epoxide resin used is the mixing of one or more in the epoxy resin such as common E44, E51;
The present invention's middle ambient cure agent fast used is the mixing of one or more in the solidifying agent such as T31 solidifying agent, thiocarbamide-polyamine condensation thing, multi-thioalcohol compound, 2-ethyl-4-methylimidazole, polymeric amide, fatty ether amine, trimellitic anhydride; The present invention's middle ambient cure promotor used is the mixing of one or more in the promotor such as 2,4,6-, tri--(dimethylamino methyl)-phenol, phenylcarbinol modified imidazole class curing catalyst, isopropylcarbinol modified imidazole class curing catalyst;
The present invention's thinner used is the mixing of one or more in ethanol, Virahol, Terpineol 350, ethylene glycol diacetate, diethylene glycol monobutyl ether, phenylcarbinol, 2-Butoxyethyl acetate, ethylene glycol, acetone, dimethyl phthalate, diethyl phthalate, phenylcarbinol and pimelinketone equal solvent;
The present invention's Mierocrystalline cellulose used is the mixing of one or more in the Mierocrystalline celluloses such as ethyl cellulose, cellulose acetate, hydroxypropylcellulose;
The present invention's defoamer used is the mixing of one or more in the materials such as higher alcohols, polypropylene glycerol aether, tributyl phosphate, silicone based defoamer;
The present invention K-570 or K-550 used is silane coupling agent, and terephthalic acid is conductivity accelerator, and nano silicon is thixotropic agent, and ICAM8401 or 8402 is stablizer;
Conductive silver glue process for preparation of the present invention is: join in epoxy resin by nano silver wire and silver powder, stir.Then add other auxiliary agent, stir deaeration when vacuum suction and mix to various material the conductive silver glue that gets product;
The feature 1 of conductive silver glue of the present invention is: conductive silver glue adopts silver powder, small part to adopt silver powder+nano silver wire as conductive filler material mostly at present.Silver powder length is less, the contact and circuit communication that thus need more silver powder to fill could to realize between silver powder.Relative to silver powder, allowed larger space between nano silver wire, thus consumption is less.Meanwhile, nano silver wire length is longer, diameter is less, and its consumption also can reduce relatively.The present invention adopts than the longer thinner nano silver wire of other products as conductive filler material, thus its silver-colored consumption less (other product silver contents 60-70%, this product 15-30%).But be not that the longer the better, oversize that it may be caused to exceed some facility is as unavailable in the width of wire casing.But the present invention's silver-colored line length used is at 30-50 μm, and its length is applicable to most occasion.Meanwhile, present invention adds conductivity accelerator, make up the conductivity decline problem brought due to space between silver-colored line, make conductive silver glue of the present invention have outstanding conductivity;
The feature 2 of conductive silver glue of the present invention is: specific epoxy resin and solidifying agent that to have selected ambient cure easily the resin that the present invention provides from lot of documents and patent and solidifying agent, makes final conductive silver glue can even ambient cure below 100 DEG C.Meanwhile, pick several efficient curing catalyst, set time is shortened greatly.But the greatest problem that middle ambient cure conductive silver glue faces is solidification value, and namely the low conductive silver glue that causes starts slowly to solidify at normal temperature, causes its stably stored time short.For this problem, present invention adds stablizer ICAM8401 or 8402 and the elargol of preparation is kept between-10-0 DEG C, the stably stored time of elargol of the present invention is promoted greatly;
The feature 3 of conductive silver glue of the present invention is: present invention adds thixotropic agent, defoamer and coupling agent, considerably increases the coating effect of elargol, improves conduction homogeneity.Add the performance such as anti-impact pressure, plasticity that Mierocrystalline cellulose improves the rear elargol product of solidification, add product competitiveness;
The invention has the advantages that: (1) silver content is low, and product cost is low; (2) product coating property is excellent, cohesiveness is strong, electroconductibility is high, impact resistance is good, storge quality is good; (3) products solidifying temperature is low, set time is short, is conducive to its practical application.
Specific embodiment
Embodiment:
Select the silver powder of the nano silver wire of long 40 μm, diameter about 35nm and 10 μm as conductive filler material, E51 epoxy resin is resin, and T31 is solidifying agent, 2,4,6-, tri--(dimethylamino methyl)-phenol is curing catalyst, and Terpineol 350 is thinner, K550 is coupling agent, terephthalic acid is conductivity accelerator, and hydroxypropylcellulose is fluidizer, and nano silicon is thixotropic agent, tributyl phosphate is defoamer, and ICAM8401 is stablizer.Slurry is specifically filled a prescription and is:
Nano silver wire, 1%;
Silver powder, 24%;
E51 epoxy resin, 20%;
T31,5%;
2,4,6-, tri--(dimethylamino methyl)-phenol, 0.5%;
Terpineol 350,2%;
K-550,2%;
Terephthalic acid, 1%;
Hydroxypropylcellulose, 43%;
Nano silicon, 1%;
Tributyl phosphate, 0.2%;
ICAM8401,0.3%;
According to the amount of 1 kilogram of elargol product, calculate the amount that often kind of auxiliary agent should add, as Terpineol 350 20g.Then these auxiliary agents are taken, for subsequent use.Nano silver wire and silver powder being joined is equipped with in the still of epoxy resin, stirs.Then add other auxiliary agent, stir deaeration when vacuum suction and mix to various material the conductive silver glue that gets product;
This conductive silver glue solidifies and completes solidification in 15 minutes at 70 DEG C, and recording its volume specific resistance is 1.2 × 10 -4Ω cm, thermal conductivity 10W/ (m.k).
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.All technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available experiment of logical analysis, reasoning, or a limited experiment and technical scheme.

Claims (10)

1. the quick-setting conductive silver glue of middle normal temperature of low-solid content, is characterized in that, its formula comprises:
Nano silver wire, 1-2%;
Flake silver powder, 13-29%;
Bisphenol A epoxide resin, 20-30%;
Ambient cure agent fast, 5-10%;
Ambient cure promotor fast, 0.5-1%;
Thinner, 1-3%;
K-570 or K-550,1-3%;
Terephthalic acid, 0.5-1%;
Mierocrystalline cellulose, 20-56.3%;
Nano silicon, 0.5-1%;
Defoamer, 0.1-0.5%;
ICAM8401 or 8402,0.1-0.5%.
2. conductive silver glue according to claim 1, is characterized in that: the length of the present invention's nano silver wire used is 30-50 μm, and diameter is 30-50nm; Flake silver powder used is 10 μm of silver powder.
3. conductive silver glue according to claim 1, is characterized in that: the present invention's bisphenol A epoxide resin used is the mixing of one or more in the epoxy resin such as common E44, E51.
4. conductive silver glue according to claim 1, is characterized in that: the present invention's middle ambient cure agent fast used is the mixing of one or more in the solidifying agent such as T31 solidifying agent, thiocarbamide-polyamine condensation thing, multi-thioalcohol compound, 2-ethyl-4-methylimidazole, polymeric amide, fatty ether amine, trimellitic anhydride.
5. conductive silver glue according to claim 1, it is characterized in that: the present invention's middle ambient cure promotor used is 2, the mixing of one or more in the promotor such as 4,6-, tri--(dimethylamino methyl)-phenol, phenylcarbinol modified imidazole class curing catalyst, isopropylcarbinol modified imidazole class curing catalyst.
6. conductive silver glue according to claim 1, is characterized in that: the present invention's thinner used is the mixing of one or more in ethanol, Virahol, Terpineol 350, ethylene glycol diacetate, diethylene glycol monobutyl ether, phenylcarbinol, 2-Butoxyethyl acetate, ethylene glycol, acetone, dimethyl phthalate, diethyl phthalate, phenylcarbinol and pimelinketone equal solvent.
7. conductive silver glue according to claim 1, is characterized in that: the present invention's Mierocrystalline cellulose used is the mixing of one or more in the Mierocrystalline celluloses such as ethyl cellulose, cellulose acetate, hydroxypropylcellulose.
8. conductive silver glue according to claim 1, is characterized in that: the present invention's defoamer used is the mixing of one or more in the materials such as higher alcohols, polypropylene glycerol aether, tributyl phosphate, silicone based defoamer.
9. conductive silver glue according to claim 1, is characterized in that: the present invention K-570 or K-550 used is silane coupling agent, and terephthalic acid is conductivity accelerator, and nano silicon is thixotropic agent, and ICAM8401 or 8402 is stablizer.
10. conductive silver glue according to claim 1, is characterized in that: conductive silver glue process for preparation of the present invention is: join in epoxy resin by nano silver wire and silver powder, stir; Then add other auxiliary agent, stir deaeration when vacuum suction and mix to various material the conductive silver glue that gets product.
CN201510646972.2A 2015-10-09 2015-10-09 A kind of middle normal temperature quick-setting conductive silver glue of low-solid content Active CN105131881B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105551571A (en) * 2016-02-01 2016-05-04 深圳市思迈科新材料有限公司 Low-temperature fast curing conductive silver paste and preparation method thereof
CN106675500A (en) * 2017-01-09 2017-05-17 成都科愿慧希科技有限公司 Ultraviolet-cured conductive silver adhesive and preparation method thereof
CN106675434A (en) * 2017-01-09 2017-05-17 成都科愿慧希科技有限公司 Conductive silver adhesive capable of being quickly cured
WO2019108732A1 (en) * 2017-12-01 2019-06-06 The Regents Of The University Of California Methods for conductive adhesives based on graphene and applications thereof
CN110890167A (en) * 2018-09-10 2020-03-17 昆山工研院新型平板显示技术中心有限公司 Conductive paste, preparation method and display device comprising conductive paste
CN114512264A (en) * 2022-02-25 2022-05-17 浙江奕成科技有限公司 Quick-drying conductive silver adhesive for display screen and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102676102A (en) * 2011-03-16 2012-09-19 上海富信新能源科技有限公司 Silver nanowire doped conductive silver colloid and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102676102A (en) * 2011-03-16 2012-09-19 上海富信新能源科技有限公司 Silver nanowire doped conductive silver colloid and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈平等: "《环氧树脂》", 31 March 1999, 化学工业出版社 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105551571A (en) * 2016-02-01 2016-05-04 深圳市思迈科新材料有限公司 Low-temperature fast curing conductive silver paste and preparation method thereof
CN106675500A (en) * 2017-01-09 2017-05-17 成都科愿慧希科技有限公司 Ultraviolet-cured conductive silver adhesive and preparation method thereof
CN106675434A (en) * 2017-01-09 2017-05-17 成都科愿慧希科技有限公司 Conductive silver adhesive capable of being quickly cured
CN106675434B (en) * 2017-01-09 2019-09-20 成都科愿慧希科技有限公司 One kind can rapid curing conductive silver glue
WO2019108732A1 (en) * 2017-12-01 2019-06-06 The Regents Of The University Of California Methods for conductive adhesives based on graphene and applications thereof
US10982119B2 (en) 2017-12-01 2021-04-20 The Regents Of The University Of California Methods for conductive adhesives based on graphene and applications thereof
CN110890167A (en) * 2018-09-10 2020-03-17 昆山工研院新型平板显示技术中心有限公司 Conductive paste, preparation method and display device comprising conductive paste
CN114512264A (en) * 2022-02-25 2022-05-17 浙江奕成科技有限公司 Quick-drying conductive silver adhesive for display screen and preparation method thereof

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Effective date of registration: 20221205

Address after: Building C, No. 888, Huanhu West 2nd Road, Lingang New District, Pudong New Area pilot Free Trade Zone, Shanghai

Patentee after: Shanghai Juerxi Electronic Technology Co.,Ltd.

Address before: 402168 Chongqing Yongchuan District double bamboo town

Patentee before: CHONGQING University OF ARTS AND SCIENCES

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